A kind of synthetic method of methoxamine hydrochloride

Abstract

A new method for synthesizing methoxamine hydrochloride, the method steps: under the protection of nitrogen, add liquid methyl p-toluenesulfonate to a certain amount of potassium carbonate in acetonitrile solution, and control the temperature to 15°C±3°C , slowly drop into the mixture of acetonitrile containing an appropriate amount of hydroquinone. Stir for another 5 minutes, heat up to 83° C. and reflux vigorously for reaction. When reflux occurs, turn off the nitrogen gas, and the reaction will be complete within 22 hours. Then through Friedel-Crafts acylation reaction, oximation reaction, oxime group reduction reaction, ketoamine hydrogenation reaction, and finally the target product was synthesized by an economical and environmentally friendly route. The yields of the 5-step operations were: 94%, 72%, 80%, 79% and 88%, respectively. The invention has the advantages of mild reaction, simple conditions, stable and easy scale-up production, and improved yield compared with the traditional synthesis of methoxamine hydrochloride.

Description

technical field [0001] The invention relates to an organic chemical synthesis method, in particular to a synthesis method of methoxamine hydrochloride. Background technique [0002] Methoxamine hydrochloride is a commonly used drug for regulating vasoconstriction and improving blood pressure. There is no report on its total synthesis in domestic literature, and foreign countries mostly use some classic reactions to study its conditions to obtain a relatively ideal yield. For example, using Dimethyl sulfate for methylation. Although it has taken a firm step forward technically, it has not taken into account its practical reality. The invention starts from the most readily available raw materials, synthesizes the target product through multi-step reactions and research on reaction conditions, and improves the reaction yield compared with the synthesis of traditional methoxamine hydrochloride. The most prominent place is the selection of methyl p-toluenesulfonate, which has n...

AI Technical Summary

Problems solved by technology

The innovations of the two have jointly promoted the development of the social economy. The former has reported that dimethyl sulfate and potassium iodide have been used as methylation reagents to achieve good results, but they are highly toxic chemical reagents and require special procedures. procedures and formalities can only be applied, which greatly limits their widespread application

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